CN100558673C - Isostatic pressing prepares the method for quartz-ceramics - Google Patents
Isostatic pressing prepares the method for quartz-ceramics Download PDFInfo
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- CN100558673C CN100558673C CNB2006100703106A CN200610070310A CN100558673C CN 100558673 C CN100558673 C CN 100558673C CN B2006100703106 A CNB2006100703106 A CN B2006100703106A CN 200610070310 A CN200610070310 A CN 200610070310A CN 100558673 C CN100558673 C CN 100558673C
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Abstract
The present invention relates to the method that a kind of isostatic pressing prepares quartz-ceramics, belong to the ceramic technology field, comprise fused quartz batching, moulding and burn till, it is characterized in that moulding adopts isostatic pressing.Adopt isostatic pressing, the blank density of moulding product is even, the intensity height, and technical process is simple, and control is convenient, and adaptability is strong, and is with short production cycle, and the production efficiency height is beneficial to and applies.
Description
Technical field
The present invention relates to a kind of preparation method of improved quartz-ceramics, belong to the ceramic technology field.
Background technology
In recent years, quartz-ceramics had obtained using widely with its excellent performance, if any finished products such as quartz-ceramics radome and quartz-ceramics damper blocks.
At present, plaster mold slip casting method is adopted in the preparation of quartz-ceramics goods more at large, also has the comparatively advanced notes of employing to coagulate the method method of forming in addition.The product surface shape that plaster mold slip casting method molds is coarse, and moulding eats that the slurry time is longer, and blank strength is low, and blank density is inhomogeneous; Annotate the method for coagulating and realize that the base substrate dead size solidifies owing to rely on the reaction of organic monomer low temperature polymerization, the factor that influences polyreaction is more, and technology controlling and process homogeneity of product and homogeneity are comparatively complicated.
Summary of the invention
The object of the present invention is to provide a kind of isostatic pressing to prepare the method for quartz-ceramics, the blank density of moulding product is even, the intensity height, and technical process is simple, and control is convenient, and adaptability is strong, and is with short production cycle, the production efficiency height.
Isostatic pressing of the present invention prepares the method for quartz-ceramics, comprises fused quartz batching, moulding and burns till, and it is characterized in that moulding adopts isostatic pressing.
It is suitable that forming pressure is controlled to be 20～300MPa.
Blank density Deng the isostatic pressing moulding is even, and the intensity height can directly be processed; But the product of moulding need not to dry direct sintering, shortens life cycle of the product greatly, and technical process is simple, the production efficiency height, and adaptability is good, can moulding large size or special-shaped product.
Among the preparation method of the present invention:
It is 0～60% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, laser particle analyzer test d
90＜60 μ m.
Preferably at first fused quartz is made slip, again reshaping behind mist projection granulating.Can be dispersion medium (quality of water be fused quartz quality 15～50%) in ball mill with fused quartz with water, add the ammonium salt class (comprising ammonium citrate, ammonium polyacrylate) of slip total mass 0.01～3% and grind dispersion agent, through grinding the preparation ceramic slurry, dispersion agent makes slip that better suspension be arranged.
In process of lapping, add the polyvinyl alcohol adhesive of fused quartz 0.01～15%.Because fused quartz is the ridge material, processability is poor, adds polyvinyl alcohol adhesive and can make quartzy material that good plasticity-is arranged, and is beneficial to moulding.
Can also add admixture in process of lapping, comprise nitride, oxide compound etc., silicon nitride and chromic oxide etc. are for example arranged, the bending strength of pottery is improved, add-on is 0～50% of a fused quartz quality.
Add pore former or/and molecular weight is 2000 polyoxyethylene glycol softening agent in process of lapping, the add-on of pore former is 5～50% of a fused quartz quality, and the softening agent add-on is 0.01～15% of a fused quartz quality.Pore former is selected polypropylene fibre, modified-cellulose etc. for use, can produce pore in sintering process, the preparation porous articles.Softening agent plays plasticizing, lubricates in powder effect.
With ceramic slurry spray-drier granulation, control process parameters: 250～300 ℃ of inlet temperatures, 110～150 ℃ of temperature outs make water ratio and are 0.2～2% quartz particles material, and granularity is that the particulate material of 80～250 mesh sieves is used for isostatic pressing.
Or with the oven dry of fused quartz slip, dry-pressing becomes piece under the pressure of 10～80MPa, and is broken again, selects the particulate material of 30 mesh sieves to be used for isostatic pressing.
Work in-process after the moulding through conventional mode burn till product, common firing temperature is 1150～1350 ℃.
Preparation method's quartz-ceramics product of the present invention, after testing, performance index: 1000 ℃ of water-cooleds of heat resistanceheat resistant stability number of times are greater than 6 times, thermal expansivity:＜1.0 * 10
-6/ ℃, bending strength is greater than 10MPa, as is used to prepare ceramic radome, its DIELECTRIC CONSTANT: 2.0～3.3 (0～500 ℃), loss tangent tg δ :≤1 * 10
-3(0～500 ℃).
Isostatic pressing of the present invention prepares the method for quartz-ceramics, and the blank density of moulding product is even, the intensity height, and technical process is simple, and control is convenient, and adaptability is strong, and is with short production cycle, and the production efficiency height is beneficial to and applies.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Fused quartz 100%, it is 40% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 45% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the slip mist projection granulating that makes, 280～290 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 1% quartz particles material, getting granularity is the material filling mould of 80～250 mesh sieves, isostatic pressing, pressure is 150MPa, and firing temperature is 1250 ± 5 ℃.The quartz-ceramics volume density that makes is 1.91g/cm
3, apparent porosity is 12.74%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 46.7MPa.
Embodiment 2
Fused quartz 100%, it is 55% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 35% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the quality of the silicon nitride that adds accounts for 0.5% of fused quartz quality, the slip mist projection granulating that makes, 280～290 ℃ of inlet temperatures, 125～135 ℃ of temperature outs make water ratio and are 1.2% quartz particles material, getting granularity is the material filling mould of 80～250 mesh sieves, isostatic pressing, pressure are 150MPa, and firing temperature is 1250 ± 5 ℃.The quartz-ceramics volume density that makes is 1.94g/cm
3, apparent porosity is 10.8%, thermal expansivity:＜1.0 * 10
-6/ ℃, bending strength is 65.7MPa, shows to add the intensity that silicon nitride can strengthen quartz-ceramics.
Embodiment 3
Fused quartz 100%, it is 30% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 35% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the quality of the chromic oxide that adds accounts for 0.5% of fused quartz quality, the slip mist projection granulating that makes, 280～290 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 1.1% quartz particles material, getting granularity is the material filling mould of 80～250 mesh sieves, isostatic pressing, pressure are 150MPa, and firing temperature is 1250 ± 5 ℃. the quartz-ceramics volume density that makes is 1.96g/cm
3, apparent porosity is 10.31%, thermal expansivity:＜1.0 * 10
-6/ ℃, bending strength is 66.5MPa, shows to add the intensity that chromic oxide can strengthen quartz-ceramics.
Embodiment 4
Fused quartz 100%, it is 35% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 25% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the quality of the polypropylene fibre pore former that adds accounts for 20% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 10MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 20MPa, firing temperature is 1250 ± 5 ℃, and the quartz-ceramics volume density that makes is 1..25g/cm
3, void content is 43.8%, the thermal expansivity of pottery:＜1.0 * 10
-6/ ℃, bending strength is 15.6MPa.
Embodiment 5
Fused quartz 100%, it is 35% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 25% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, molecular weight is that 2000 polyoxyethylene glycol softening agent accounts for 5% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 50MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 150MPa, and firing temperature is 1250 ± 5 ℃.The quartz-ceramics volume density that makes is 1.84g/cm
3, apparent porosity is 15.21%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 43.7MPa.
Embodiment 6
Fused quartz 100%, it is 35% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 45% of fused quartz quality in the ball mill, the ammonium citrate dispersion agent accounts for 1.5% of slip, polyvinyl alcohol adhesive accounts for 0.8% of fused quartz quality, the slip mist projection granulating that makes, 280～290 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 1.4% quartz particles material, getting granularity is the material filling mould of 80～250 mesh sieves, isostatic pressing, pressure is 200MPa, and firing temperature is 1280 ± 5 ℃.The quartz-ceramics volume density that makes is 1.96g/cm
3, apparent porosity is 10.34%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 67.5MPa.
Embodiment 7
Fused quartz 100%, it is 48% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 18% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2.5% of slip, polyvinyl alcohol adhesive accounts for 8% of fused quartz quality, the quality of the silicon nitride that adds accounts for 5% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 60MPa, selected the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 180MPa, and firing temperature is 1180 ± 5 ℃.The quartz-ceramics volume density that makes is 1.63g/cm
3, apparent porosity is 25.51%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 34.4MPa.
Embodiment 8
Fused quartz 100%, it is 15% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 28% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 10% of fused quartz quality, the quality of the chromic oxide that adds accounts for 3% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 70MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 250MPa, and firing temperature is 1230 ± 5 ℃.The quartz-ceramics volume density that makes is 1.54g/cm
3, apparent porosity is 29.15%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 25.9MPa.
Embodiment 9
Fused quartz 100%, it is 30% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 25% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 1.5% of slip, polyvinyl alcohol adhesive accounts for 1% of fused quartz quality, the quality of the modified-cellulose pore former that adds accounts for 30% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 20MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 50MPa, and firing temperature is 1320 ± 5 ℃.The quartz-ceramics volume density that makes is 1.24g/cm
3, apparent porosity is 44.8%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 14.6MPa.
Embodiment 10
Fused quartz 100%, it is 52% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 22% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 6% of fused quartz quality, molecular weight is that 2000 polyoxyethylene glycol softening agent accounts for 8% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 50MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 150MPa, and firing temperature is 1250 ± 5 ℃.The quartz-ceramics volume density that makes is 1.75g/cm
3, apparent porosity is 19.89%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 37.2MPa.
Embodiment 11
Fused quartz 100%, it is 50% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, the ball mill WATER AS FLOW MEDIUM accounts for 30% of fused quartz quality, and the ammonium citrate dispersion agent accounts for 1.6% of slip, and polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 50MPa, the material of getting 30 mesh sieves loads mould, isostatic pressing, pressure is 200MPa, and firing temperature is 1290 ± 5 ℃.The quartz-ceramics volume density that makes is 1.90g/cm
3, apparent porosity is 13.23%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 45.9MPa.
Embodiment 12
Fused quartz 100%, it is 48% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 25% of fused quartz quality in the ball mill, the ammonium citrate dispersion agent accounts for 0.9% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the quality of the modified-cellulose pore former that adds accounts for 3% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 60MPa, selected the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 180MPa, and firing temperature is 1170 ± 5 ℃.The quartz-ceramics volume density that makes is 1.82g/cm
3, apparent porosity is 15.93%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 41.6MPa.
Embodiment 13
Fused quartz 100%, it is 33% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 28% of fused quartz quality in the ball mill, the ammonium citrate dispersion agent accounts for 2.2% of slip, polyvinyl alcohol adhesive accounts for 4% of fused quartz quality, the quality of the chromic oxide that adds accounts for 3% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 80MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 230MPa, and firing temperature is 1230 ± 5 ℃.The quartz-ceramics volume density that makes is 1.96g/cm
3, apparent porosity is 10.45%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 68.2MPa.
Embodiment 14
Fused quartz 100%, it is 42% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 50% of fused quartz quality in the ball mill, the ammonium polyacrylate dispersion agent accounts for 1.3% of slip, polyvinyl alcohol adhesive accounts for 1% of fused quartz quality, the quality of the modified-cellulose pore former that adds accounts for 25% of fused quartz quality, the slip mist projection granulating that makes, 275～285 ℃ of inlet temperatures, 125～135 ℃ of temperature outs make water ratio and are 1.5% quartz particles material, getting granularity is the material filling mould of 80～250 mesh sieves, isostatic pressing, pressure are 220MPa, and firing temperature is 1310 ± 5 ℃.The quartz-ceramics volume density that makes is 1.21g/cm
3, apparent porosity is 46.7%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 13.5MPa.
Embodiment 15
Fused quartz 100%, it is 52% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 22% of fused quartz quality in the ball mill, the ammonium citrate dispersion agent accounts for 6% of slip, polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, molecular weight is that 2000 polyoxyethylene glycol softening agent accounts for 4% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 60MPa, got the material filling mould of 30 mesh sieves, isostatic pressing, pressure are 190MPa, and firing temperature is 1260 ± 5 ℃.The quartz-ceramics volume density that makes is 1.87g/cm
3, apparent porosity is 14.02%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 45.3MPa.
Embodiment 16
Fused quartz 100%, it is 0% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 40% of fused quartz quality in the ball mill, and the ammonium citrate dispersion agent accounts for 2% of slip, and polyvinyl alcohol adhesive accounts for 5% of fused quartz quality, the slip oven dry back that makes is broken, broken behind the pressurization 50MPa, the material of getting 30 mesh sieves loads mould, isostatic pressing, pressure is 110MPa, and firing temperature is 1250 ± 5 ℃.The quartz-ceramics volume density that makes is 1.96g/cm
3, apparent porosity is 10.25%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 68.2MPa.
Embodiment 17
Fused quartz 100%, it is 22% of fused quartz total masses to the quality of 325 mesh sieves that the fused quartz grain diameter is controlled at 150 mesh sieves, dispersion medium water accounts for 40% of fused quartz quality in the ball mill, the ammonium citrate dispersion agent accounts for 2% of slip, polyvinyl alcohol adhesive accounts for 4% of fused quartz quality, the slip mist projection granulating that makes, 280～285 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 0.8% quartz particles material, getting granularity is the material filling mould of 80～250 mesh sieves, isostatic pressing, pressure is 110MPa, and firing temperature is 1250 ± 5 ℃.The quartz-ceramics volume density that makes is 1.93g/cm
3, apparent porosity is 11.12%, thermal expansivity is＜1.0 * 10
-6/ ℃, bending strength is 51.2MPa.
Claims (1)
1, a kind of isostatic pressing prepares the method for quartz-ceramics, comprises fused quartz batching, moulding and burns till, and it is characterized in that moulding adopts isostatic pressing, and forming pressure is 20～300MPa;
The fused quartz grain diameter is 15～60% of fused quartz total masses at 150 mesh sieves to the quality of 325 mesh sieves;
At first fused quartz is made slip, with fused quartz is to grind dispersion medium in ball mill with water, add the ammonium salt class dispersion agent of slip total mass 0.01～3%, through grinding the preparation ceramic slurry, add the polyvinyl alcohol adhesive of fused quartz 0.01～15% in the process of lapping, add pore former or/and molecular weight is 2000 polyoxyethylene glycol softening agent, the add-on of pore former is 5～50% of a fused quartz quality, and the softening agent add-on is 0.01～15% of a fused quartz quality; With ceramic slurry spray-drier granulation, control process parameters: 250～300 ℃ of inlet temperatures, 110～150 ℃ of temperature outs make water ratio and are 0.2～2% quartz particles material, and the particulate material of choosing granularity and be 80～250 mesh sieves is used for isostatic pressing.
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| CN103553580B (en) * | 2013-10-16 | 2014-11-05 | 徐州协鑫太阳能材料有限公司 | Insulating magnetic ring for polysilicon reduction furnace and manufacturing method thereof |
| CN111718197A (en) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | Thin quartz ceramic component and efficient preparation method thereof |
| CN112939588B (en) * | 2021-04-08 | 2023-01-24 | 中国轻工业陶瓷研究所 | Method for preparing material with high thermal expansion coefficient by utilizing industrial waste through microwave heating |
| CN115340394A (en) * | 2022-08-10 | 2022-11-15 | 武汉科技大学 | Boron phosphate reinforced quartz material and preparation method thereof |
| CN116874292A (en) * | 2023-08-03 | 2023-10-13 | 西安交通大学 | High-strength high-purity silicon dioxide ceramic and manufacturing method thereof |
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